CN103387518A - Preparation method of N,N-dimethylglycine - Google Patents
Preparation method of N,N-dimethylglycine Download PDFInfo
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Abstract
The invention relates to a preparation method of N,N-dimethylglycine and belongs to the field of chemical engineering. The preparation method comprises the following steps of: preparing N,N-dimethyl amino acetonitrile by taking hydroxyacetonitrile and dimethylamine as raw materials, obtaining an N,N-dimethylglycine crude product by alkalizing the reaction liquid with an inorganic base and neutralizing the reaction liquid with an organic acid on the basis of N,N-dimethyl amino acetonitrile reaction liquid, and finally separating and purifying the N,N-dimethylglycine crude product to obtain the high-quality N,N-dimethylglycine product. The preparation method has the advantages that the raw materials are environmentally-friendly and easily available, reaction conditions are mild, the environmental pollution is little, the after-treatment is simple and easy, the production efficiency is high, and the preparation method is suitable for industrial popularization and application.
Description
Technical field
The present invention is directed to chemical field, relate to a kind of preparation method of DMG, be specifically related to utilize N, N-dimethylamino acetonitrile prepares the method for DMG.
Background technology
DMG (N-dimethyl glycine, be called for short DMG for Dimethyl glycine, N, and namely VITMAIN B1 6), outward appearance is white crystals, water-soluble and ethanol.Can be used for the treatment of person in middle and old age's melancholia as medicine, stimulate Human immune responses, reduce the injury of public hazards pollutent to health, reduce body inner cholesterol content etc.In addition, in food service industry, can be used as oxidation inhibitor, in pharmaceutical industries, can be used as medicine intermediate, synthetic multiple biochemical drug.
Patent US4968839 has reported the synthetic process of DMG, is about to dimethylamine and formaldehyde, sodium cyanide, sodium bisulfite effect and makes the dimethylamino acetonitrile, and then alkaline hydrolysis, obtain the product DMG after neutralization.The sodium cyanide of severe toxicity is arranged in the method raw material, can impact environment, be difficult for promoting the use of, and yield is only also 66% left and right.
Yu Hongxia etc. reported a kind of take glycine as raw material, Pd/C as catalyzer prepare DMG method (Yu Hongxia, Guo Feng .N, the study on the synthesis of N-N-methylsarcosine. Tianjin chemical industry, 2004,18 (4): 38-39).Although the yield of the method DMG increases, the Pd/C catalyzer that uses is very expensive, also is not suitable for industry and promotes.
In addition, Zhu Xiaohui etc. have reported a kind of processing method of producing DMG, and this processing method is with making calcium chloroacetate with the Mono Chloro Acetic Acid aqueous solution in calcium hydroxide, filter and remove insoluble impurities, then with the condensation of diformazan ammonia, the feed liquid warp is concentrated, acidifying, filtration makes N, the N-dimethyl glycine hydrochloride (Zhu Xiaohui, Zhang Gongxiao. synthesizing of dimethyl glycine hydrochloride. Taishan Hospital's journal, 2004 25 (6): 649-650).Though the method has become the main flow technique of DMG preparation, what obtain is the hydrochloride of DMG, still is restricted in application.
For these reasons and prior art, still need to be optimized the preparation of DMG, especially this preparation method is in security consideration, yield improve, industry is promoted consideration.The present invention is directed to the deficiencies in the prior art and carried out improving invention.
Summary of the invention
In view of this, the invention provides a kind of N, N-dimethylamino acetonitrile is as preparation N, the intermediate of N-N-methylsarcosine, this intermediate prepare required raw material environmental protection and are easy to get, and reaction conditions is gentle, the reaction solution of gained need not separate, and can be further used for the preparation of DMG.
For achieving the above object, technical scheme of the present invention is:
A kind of N, the preparation method of N-dimethylamino acetonitrile comprises the following steps:
Hydroxyacetonitrile and excessive dimethylamine fully react to obtain N, the reaction solution of N-dimethylamino acetonitrile in water medium.Reaction formula is as follows:
Further, the temperature of described reaction is 40～100 ℃, and pressure is 0.4～1MPa.Described hydroxyacetonitrile: the mol ratio of dimethylamine is 1:1.5～4, preferred 1:1.5～2.Preferred 60～80 ℃ of described temperature of reaction.Preferred 0.5～1 hour of described reaction times.Preferred 0.6～the 0.8MPa of described reaction pressure.
In this preparation method, the recyclable recycling of unnecessary dimethylamine, reclaim as the mode by heating evaporation.
Obtaining N, on the basis of N-dimethylamino acetonitrile reaction solution, further prepare DMG salt, comprise the following steps: the N that obtains to claim 1, add N in N-dimethylamino acetonitrile reaction solution, the alkali of 0.7～2 times of molar weight of N-dimethylamino acetonitrile alkalizes, and controls 60～100 ℃ of temperature of reaction, reacted 2～7 hours, after deamination is processed, obtain the reaction solution of DMG salt.Reaction formula following (mineral alkali is take sodium hydroxide as example):
Further, described alkali is one or more in sodium hydroxide, potassium hydroxide, hydrated barta, calcium oxide, sodium sulfate, ammonium sulfate and calcium hydroxide.The consumption of described mineral alkali, preferred 1～1.5 times of N, the molar weight of N-dimethylamino acetonitrile.Preferred 60～85 ℃ of described temperature of reaction.
Another object of the present invention is to provide a kind of N, the preparation method of N-N-methylsarcosine, this method is at N, carry out on the basis of the reaction solution of N-N-methylsarcosine salt, the method reaction conditions is gentle, and environmental pollution is little, aftertreatment is simple and easy, product yield is high, and the intermediate product reusable edible, and suitable industry is applied.
N, the preparation method of N-N-methylsarcosine, at described N, on the reaction solution basis of N-N-methylsarcosine salt, to adding acid for adjusting pH in the reaction solution of DMG salt, be acid, obtain N, the mixed solution of N-N-methylsarcosine crude product and inorganic salt, obtain DMG to this mixed solution separation and purification.Reaction formula following (acid is take sulfuric acid as example):
The common purifying of described separation comprises the following steps: to N, add 0.05～2% gac in the mixed solution of N-N-methylsarcosine crude product and inorganic salt, decoloured 0.5～1 hour, the centrifugal gac of removing, obtain mother liquor 1 and be cooled to 10 ℃ of crystallizations, the centrifugal inorganic salt of removing, obtain mother liquor 2 recrystallizations, the centrifugal DMG that namely obtains again.The present invention can be routinely the crystallization purifying method to the N of above-mentioned acquisition, the N-N-methylsarcosine is recrystallization repeatedly, to obtain the higher N of purity, N-N-methylsarcosine elaboration, and this N, the mother liquor 2 that mother liquor 3 after the crystallization of N-N-methylsarcosine can be incorporated into next round production carries out crystallization, improves product yield.
Further, described acid is mineral acid, one or more in preferably sulfuric acid, hydrochloric acid, nitric acid, carbonic acid, phosphoric acid and Lewis acid, preferably sulfuric acid or hydrochloric acid.Lewis acid commonly used is any or multiple in the fluoroform sulphonate of aluminum chloride, iron(ic) chloride, boron trifluoride, columbium pentachloride and lanthanon.
Further, described acid for adjusting pH is 5 ± 0.5.
In addition, the reaction solution of described DMG salt also can prepare in accordance with the following methods, the method comprises the following steps: formaldehyde, sodium cyanide, dimethylamine are in water medium, and after 60～80 ℃ of abundant reactions of temperature, deamination is processed, obtain the reaction solution of DMG sodium; In water medium, formaldehyde: sodium cyanide: the mol ratio of dimethylamine is 1:1～1.5:1.5～3.Reaction formula is as follows:
Further, the reaction times of described reaction is 0.5～5 hour.Described formaldehyde: sodium cyanide: the preferred 1:1.1:2 of the mol ratio of dimethylamine.
While including the step that ammonia emits in above-mentioned reaction, the maintenance reaction system is negative pressure, helps overflowing of ammonia, and the ammonia of emitting can pass through water or sulfuric acid absorption.
Another kind of preparation method, relate in specific recycle unit and produce DMG, namely utilizes the DMG production equipment to prepare the method for DMG.As shown in Figure 1, described DMG production equipment comprises 101# reactor, 102# reactor, 2# reactor, tripping device and crystallization kettle; Described 101# reactor and 102# reactor are communicated with the 2# reactor respectively; Described tripping device is whizzer or filtration unit, and is communicated with 2# reactor and crystallization kettle respectively;
A, hydroxyacetonitrile, excessive dimethylamine and water fully react to obtain N, the reaction solution of N-dimethylamino acetonitrile in 101# reactor (1); To N, add N in N-dimethylamino acetonitrile reaction solution, the alkali alkalization of 0.7～2 times of molar weight of N-dimethylamino acetonitrile, control 60～100 ℃ of temperature of reaction, reacted 2～7 hours, after deamination is processed, obtains the reaction solution of DMG salt;
Perhaps, formaldehyde, sodium cyanide, dimethylamine and water are in 102# reactor (2), and after 60～80 ℃ of abundant reactions of temperature, deamination is processed, and obtains the reaction solution of DMG sodium; In water medium, formaldehyde: sodium cyanide: the mol ratio of dimethylamine is 1:1～1.5:1.5～3;
B, change the reaction solution in 101# reactor (1) and/or 102# reactor (2) over to 2# reactor (3), it is acid adding wherein acid for adjusting pH, then adds activated carbon decolorizing, obtains mixtures of materials;
C, change the mixtures of materials in reactor over to tripping device and separate, obtain mother liquor 1;
D, change described mother liquor 1 over to the crystallization kettle crystallisation by cooling, then by tripping device, separate to obtain solids inorganic salt and mother liquor 2;
E, change described mother liquor 2 over to the crystallization kettle recrystallization, then by tripping device, separate to obtain DMG and mother liquor 3.
Further, described mother liquor 3 changes crystallization kettle over to, with lower whorl mother liquor 2, mixes recrystallization in the lump, further prepares DMG.The DMG that obtains can further improve purity by recrystallization repeatedly.
According to the reaction requirement, described 101# reactor should be autoclave.102# reactor, 2# reactor and crystallization kettle are completed in reaction function, can be completed by a reactor in theory, can heat or lower the temperature by the interlayer to reactor logical steam, hot water or icy salt solution etc.Relate to deamination in 101# reactor and 102# reactor reaction process and process, can corresponding outfit ammonia absorption device, can fill the absorption for ammonia of water or sulfuric acid in this device.
The invention has the beneficial effects as follows:
N of the present invention, the preparation method of N-N-methylsarcosine, first adopt hydroxyacetonitrile and dimethylamine to prepare N, N-dimethylamino acetonitrile, pass through N, N-dimethylamino acetonitrile alkaline hydrolysis, neutralization, purifying successively obtains the DMG elaboration again, the intermediate product of each step need not to separate with reaction solution, can carry out next step operation.N, the alkaline hydrolysis step of N-dimethylamino acetonitrile is directly carried out its reaction solution, has both guaranteed that hydrolysis is thorough, has avoided again the side reaction in the deamination process.Neutralization procedure has used comparatively cheap electrodeless acid to be raw material, reduce production costs simultaneously, by-product inorganic salts after neutralization can be used for again other industrial reaction, and, can choosing according to the mineral acid kind, selectively control chlorion and other negatively charged ion, can also disposablely according to customer demand prepare with high yield the DMG crude product that contains certain inorganic salt.In addition, present method ingenious dissolubility difference that utilizes DMG and inorganic salt also, can realize effective separation, wherein, a front N, mother liquor after the crystallization of N-N-methylsarcosine is the crystallization to next DMG crude product capable of circulation also, and raw material is fully used.Confirm through embodiment, the DMG yield of acquisition can reach 91%, purity 99%.
To sum up, preparation method's raw material environmental protection of DMG of the present invention is easy to get, and reaction conditions is gentle, and environmental pollution is little, and aftertreatment is simple and easy, and production efficiency is high, and suitable industry is applied.
Description of drawings
Fig. 1 is DMG production equipment structural representation.
Embodiment
Hereinafter with reference to accompanying drawing, the preferred embodiments of the present invention are described in detail.The experimental technique of unreceipted actual conditions in preferred embodiment, usually according to normal condition.
The standby DMG of embodiment 1 hydroxyacetonitrile legal system
at room temperature, add the 1000g40% hydroxyl acetonitrile aqueous solution in high-pressure reactor, then pass into the 1435g33% dimethylamine agueous solution, be warming up to 60 ℃, pressure 0.7MPa, react after 0.5 hour, stopped reaction, reaction solution is changed in the flask of 3000ml, again to the aqueous sodium hydroxide solution that adds 561g50% in reaction solution, in 80 ℃ of insulations 5 hours, obtain N, the ammonia solution of N-N-methylsarcosine sodium salt, deamination obtains N, N-N-methylsarcosine sodium salt solution, add subsequently 98% sulphur acid for adjusting pH to 5.0, obtain N, the mixed solution of N-N-methylsarcosine and sodium sulfate.Add the 8g activated carbon decolorizing, suction filtration is removed gac, and filtrate is cooled to 10 ℃, crystallization, the centrifugal sodium sulfate crystal of removing, filtrate crystallization purifying according to a conventional method can obtain DMG, obtain white solid 658g after super-dry, purity reaches more than 99%, and yield reaches 90%.
The standby DMG of embodiment 2 hydroxyacetonitrile legal systems
at room temperature, add the 1000g40% hydroxyl acetonitrile aqueous solution in high-pressure reactor, then pass into the 1435g33% dimethylamine agueous solution, be warming up to 60 ℃, pressure 0.7MPa, react after 0.5 hour, stopped reaction, reaction solution is changed in the flask of 3000ml, again to the potassium hydroxide aqueous solution that adds 786g50% in reaction solution, in 80 ℃ of insulations 5 hours, obtain N, the ammonia solution of N-N-methylsarcosine sylvite, deamination obtains N, N-N-methylsarcosine potassium salt soln, add subsequently 37% salt acid for adjusting pH to 5.0, obtain N, the mixed solution of N-N-methylsarcosine and Repone K.Add the 7g activated carbon decolorizing, suction filtration is removed gac, and filtrate is cooled to 10 ℃, crystallization, the centrifugal potassium chloride of removing, filtrate crystallization purifying according to a conventional method can obtain DMG, obtain white solid 665g after super-dry, purity reaches more than 99%, and yield reaches 91%.
The standby DMG of embodiment 3 hydroxyacetonitrile legal systems
at room temperature, add the 1000g40% hydroxyl acetonitrile aqueous solution in high-pressure reactor, then pass into the 1435g33% dimethylamine agueous solution, be warming up to 60 ℃, pressure 0.6MPa, react after 0.5 hour, stopped reaction, reaction solution is changed in the flask of 3000ml, again to the aqueous solution that adds in reaction solution 497g sodium sulfate and 259g calcium hydroxide to form, in 85 ℃ of insulations 7 hours, obtain N, the ammonia solution of N-N-methylsarcosine sodium salt, deamination obtains N, N-N-methylsarcosine sodium salt solution, add subsequently 37% salt acid for adjusting pH to 4.5, obtain N, the N-N-methylsarcosine, the mixed solution of sodium-chlor and calcium sulfate.Add the 8g activated carbon decolorizing, suction filtration is removed gac, filtrate is cooled to 10 ℃, crystallization, centrifugal sodium-chlor and the calcium sulphate crystal removed, filtrate crystallization purifying according to a conventional method can obtain N, the N-N-methylsarcosine, obtain white solid 661g after super-dry, purity reaches more than 98.5%, and yield reaches 90%.
The standby DMG of embodiment 4 hydroxyacetonitrile legal systems
at room temperature, add the 1000g40% hydroxyl acetonitrile aqueous solution in high-pressure reactor, then pass into the 1435g33% dimethylamine agueous solution, be warming up to 40 ℃, pressure 1MPa, react after 1 hour, stopped reaction, reaction solution is changed in the flask of 3000ml, again to the aqueous sodium hydroxide solution that adds 561g50% in reaction solution, in 95 ℃ of insulations 2 hours, obtain N, the ammonia solution of N-N-methylsarcosine sodium salt, deamination obtains N, N-N-methylsarcosine sodium salt solution, be 5.5 with adding concentrated hydrochloric acid to be acidified to pH value of solution in backward this solution, obtain N, the N-N-methylsarcosine, the mixed solution of sodium-chlor.Add the 7g activated carbon decolorizing, suction filtration is removed gac, and filtrate is cooled to 10 ℃, crystallization, the centrifugal sodium chloride crystal of removing, filtrate crystallization purifying according to a conventional method can obtain DMG, obtain white solid 672g after super-dry, purity reaches more than 99%, and yield reaches 92%.
The standby DMG of embodiment 5 hydroxyacetonitrile legal systems
at room temperature, add the 1000g40% hydroxyl acetonitrile aqueous solution in high-pressure reactor, then pass into the 1435g33% dimethylamine agueous solution, be warming up to 60 ℃, pressure 0.7MPa, react after 0.5 hour, stopped reaction, reaction solution is changed in the flask of 3000ml, again to the aqueous sodium hydroxide solution that adds 561g50% in reaction solution, in 80 ℃ of insulations 5 hours, obtain N, the ammonia solution of N-N-methylsarcosine sodium salt, deamination obtains N, N-N-methylsarcosine sodium salt solution, add subsequently 98% sulphur acid for adjusting pH to 5.0, obtain N, the mixed solution of N-N-methylsarcosine and sodium sulfate.Add the 8g activated carbon decolorizing, suction filtration is removed gac, and filtrate is cooled to 10 ℃, crystallization, the centrifugal sodium sulfate crystal of removing, filtrate crystallization purifying according to a conventional method can obtain DMG, obtain white solid 660g after super-dry, purity reaches more than 98%, and yield reaches 90%.
The standby DMG of embodiment 6 formaldehyde, sodium cyanide and dimethylamine legal system
Add 565 gram 37% formalins and 2215 gram 30% sodium cyanide solutions in reactor, then slowly drip 3363 gram 33% dimethylamine agueous solutions, dropwise, be warming up to 80 ℃, reacted 5 hours, obtain the ammonia solution of DMG sodium salt, deamination obtains N, N-N-methylsarcosine sodium salt solution, add subsequently 98% sulphur acid for adjusting pH to 5.0, obtain the mixed solution of DMG and sodium sulfate.Add 6 gram activated carbon decolorizings, suction filtration is removed gac, and filtrate is cooled to 10 ℃, crystallization, and the centrifugal sodium sulfate crystal of removing, filtrate crystallization purifying according to a conventional method can obtain DMG solid 646 grams, and purity reaches more than 99%, and yield reaches 89%.
Embodiment 7 utilizes the DMG production equipment to prepare DMG
As shown in Figure 1, this production equipment comprises 101# reactor 1,2# reactor 3, tripping device 4 and crystallization kettle 5; Tripping device 4 is the suction filtration machine, and is communicated with 2# reactor 3 and crystallization kettle 5 respectively;
A, at room temperature, add the 100kg40% hydroxyl acetonitrile aqueous solution in 101# reactor 1, then pass into the 143.5kg33% dimethylamine agueous solution, is warming up to 60 ℃, and pressure 0.7MPa, react after 0.5 hour stopped reaction; , to the aqueous sodium hydroxide solution that adds 56.1gk50% in reaction solution,, in 80 ℃ of insulations 5 hours, obtain the ammonia solution of DMG sodium salt again, deamination obtains the DMG sodium salt solution;
B, change the reaction solution in 101# reactor 1 over to 2# reactor 3, add wherein 98% sulphur acid for adjusting pH to 5.0, obtain the mixed solution of DMG and sodium sulfate; Add the 800g activated carbon decolorizing, obtain mixtures of materials;
C, change the mixtures of materials in reactor 3 over to suction filtration machine suction filtration, obtain mother liquor 1;
D, change mother liquor 1 over to crystallization kettle 5, be cooled to 10 ℃, crystallization, then change suction filtration machine suction filtration over to and remove sodium sulfate crystal, obtain mother liquor 2;
E, change mother liquor 2 over to crystallization kettle 5 recrystallization according to a conventional method, then change the suction filtration machine over to and separate to obtain DMG and mother liquor 3.
The final DMG solid 66.9kg that obtains, purity reaches more than 99%, and yield reaches 92%.Mother liquor 3 can change crystallization kettle 5 over to, with lower whorl mother liquor 2, mixes recrystallization in the lump, further prepares DMG.
Explanation is finally, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, although with reference to preferred embodiment, the present invention is had been described in detail, those of ordinary skill in the art is to be understood that, can modify or be equal to replacement technical scheme of the present invention, and not breaking away from aim and the scope of technical solution of the present invention, it all should be encompassed in the middle of claim scope of the present invention.
Claims (11)
1. N, the preparation method of N-dimethylamino acetonitrile system comprises the following steps:
Hydroxyacetonitrile and excessive dimethylamine fully react to obtain N, the reaction solution of N-dimethylamino acetonitrile in water medium.
2. N according to claim 1, the preparation method of N-dimethylamino acetonitrile system is characterized in that: the temperature of described reaction is 40～100 ℃, pressure is 0.4～1MPa.
3. N according to claim 1, the preparation method of N-dimethylamino acetonitrile system is characterized in that: described hydroxyacetonitrile: the mol ratio of dimethylamine is 1:1.5～4.
4. utilize preparation method claimed in claim 1 to prepare the method for DMG salt system, it is characterized in that: comprise the following steps:
To the N that claim 1 obtains, add N in N-dimethylamino acetonitrile reaction solution, the alkali of 0.7～2 times of molar weight of N-dimethylamino acetonitrile alkalizes, control 60～100 ℃ of temperature of reaction, reacted 2～7 hours, after deamination is processed, obtain the reaction solution of DMG salt.
5. the method for preparing the DMG salt system according to claim 4, it is characterized in that: described alkali is one or more in sodium hydroxide, potassium hydroxide, hydrated barta, calcium oxide, sodium sulfate, ammonium sulfate and calcium hydroxide.
6. N, the preparation method of N-N-methylsarcosine, it is characterized in that: on the basis of claim 4, N to gained, it is acid adding acid for adjusting pH in the reaction solution of N-N-methylsarcosine salt, obtains the mixed solution of DMG crude product and inorganic salt, this mixed solution separation and purification is obtained DMG.
7. the preparation method of DMG according to claim 6, it is characterized in that: described acid is one or more in sulfuric acid, hydrochloric acid, nitric acid, carbonic acid, phosphoric acid and Lewis acid.
8. the preparation method of DMG according to claim 6, it is characterized in that: described acid for adjusting pH is 5 ± 0.5.
9. N according to claim 6, the preparation method of N-N-methylsarcosine, it is characterized in that: described N, the reaction solution of N-N-methylsarcosine salt prepares by the following method, the method comprises the following steps: formaldehyde, sodium cyanide, dimethylamine are in water medium, and after 60～80 ℃ of abundant reactions of temperature, deamination is processed, obtain the reaction solution of DMG sodium; In water medium, formaldehyde: sodium cyanide: the mol ratio of dimethylamine is 1:1～1.5:1.5～3.
10. utilize N, N-N-methylsarcosine production equipment prepares N, the method of N-N-methylsarcosine, it is characterized in that: described DMG production equipment comprises 101# reactor (1), 102# reactor (2), 2# reactor (3), tripping device (4) and crystallization kettle (5); Described 101# reactor (1) and 102# reactor (2) are communicated with 2# reactor (3) respectively; Described tripping device (4) is whizzer or filtration unit, and is communicated with 2# reactor (3) and crystallization kettle (5) respectively;
A, hydroxyacetonitrile, excessive dimethylamine and water fully react to obtain N, the reaction solution of N-dimethylamino acetonitrile in 101# reactor (1); To N, add N in N-dimethylamino acetonitrile reaction solution, the alkali alkalization of 0.7～2 times of molar weight of N-dimethylamino acetonitrile, control 60～100 ℃ of temperature of reaction, reacted 2～7 hours, after deamination is processed, obtains the reaction solution of DMG salt;
Perhaps, formaldehyde, sodium cyanide, dimethylamine and water are in 102# reactor (2), and after 60～80 ℃ of abundant reactions of temperature, deamination is processed, and obtains the reaction solution of DMG sodium; In water medium, formaldehyde: sodium cyanide: the mol ratio of dimethylamine is 1:1～1.5:1.5～3;
B, change the reaction solution in 101# reactor (1) and/or 102# reactor (2) over to 2# reactor (3), it is acid adding wherein acid for adjusting pH, then adds activated carbon decolorizing, obtains mixtures of materials;
C, change the mixtures of materials in reactor (3) over to tripping device (4) and separate, obtain mother liquor 1;
D, change described mother liquor 1 over to crystallization kettle (5) crystallisation by cooling, then by tripping device (4), separate to obtain solids inorganic salt and mother liquor 2;
E, change described mother liquor 2 over to crystallization kettle (5) recrystallization, then by tripping device (4), separate to obtain DMG and mother liquor 3.
11. the method for utilizing the DMG production equipment to prepare DMG according to claim 10, it is characterized in that: described mother liquor 3 changes crystallization kettle (5) over to, mix recrystallization in the lump with lower whorl mother liquor 2, further prepare DMG.
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| CN104610078A (en) * | 2014-10-27 | 2015-05-13 | 河北诚信有限责任公司 | Method for preparing high-purity N,N-dimethyl glycine |
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| US9573808B2 (en) | 2013-07-31 | 2017-02-21 | Schlumberger Technology Corporation | Aqueous solution and method for use thereof |
| US9796490B2 (en) | 2013-10-24 | 2017-10-24 | Schlumberger Technology Corporation | Aqueous solution and method for use thereof |
| CN107573253A (en) * | 2017-10-25 | 2018-01-12 | 广州英赛特生物技术有限公司 | N, N dimethylglycine organic acid conjugation hydrochlorate and combinations thereof and application |
| US9920606B2 (en) | 2013-07-31 | 2018-03-20 | Schlumberger Technology Corporation | Preparation method, formulation and application of chemically retarded mineral acid for oilfield use |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US9573808B2 (en) | 2013-07-31 | 2017-02-21 | Schlumberger Technology Corporation | Aqueous solution and method for use thereof |
| US9920606B2 (en) | 2013-07-31 | 2018-03-20 | Schlumberger Technology Corporation | Preparation method, formulation and application of chemically retarded mineral acid for oilfield use |
| US9796490B2 (en) | 2013-10-24 | 2017-10-24 | Schlumberger Technology Corporation | Aqueous solution and method for use thereof |
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| CN107573253A (en) * | 2017-10-25 | 2018-01-12 | 广州英赛特生物技术有限公司 | N, N dimethylglycine organic acid conjugation hydrochlorate and combinations thereof and application |
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